CN110117416B - Ti 2 C 3 Electromagnetic shielding composite material of/para-aramid nano-fiber and preparation method thereof - Google Patents

Ti 2 C 3 Electromagnetic shielding composite material of/para-aramid nano-fiber and preparation method thereof Download PDF

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CN110117416B
CN110117416B CN201910318277.1A CN201910318277A CN110117416B CN 110117416 B CN110117416 B CN 110117416B CN 201910318277 A CN201910318277 A CN 201910318277A CN 110117416 B CN110117416 B CN 110117416B
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fiber
electromagnetic shielding
dispersion liquid
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陆赵情
贾峰峰
骆志荣
谢璠
王瑾
司联蒙
姚成
张楠
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Zhejiang Kingdecor Paper Industry Co ltd
Shaanxi University of Science and Technology
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Zhejiang Kingdecor Paper Industry Co ltd
Shaanxi University of Science and Technology
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Abstract

The invention relates to Ti 2 C 3 The preparation method of the/para-aramid nano-fiber electromagnetic shielding composite material comprises the step 1 of mixing Ti 2 C 3 Mixing the dispersion liquid and the para-aramid nano-fiber dispersion liquid, and performing ultrasonic treatment to obtain a mixed system A, wherein the mass of the para-aramid nano-fiber is Ti 2 C 3 And 3% -9% of the total mass of the para-aramid nano-fiber; step 2, sequentially carrying out vacuum-assisted filtration and hot-pressing drying on the mixed system A to obtain the material; vacuum-assisted filtration can ensure that the electromagnetic shielding composite material forms a microscopic layered structure, hot-press drying can ensure that the mechanical strength of the composite material is improved under the condition of not changing the physical properties of the material, so that the two raw materials are well subjected to interface combination, the strength of the material is improved and the electromagnetic shielding performance is regulated and controlled while certain electrical conductivity is ensured, and reference is provided for electromagnetic shielding research of electronic products.

Description

Ti 2 C 3 Electromagnetic shielding composite material of/para-aramid nano-fiber and preparation method thereof
Technical Field
The invention belongs to the crossing field of paper industry and electromagnetic shielding materials, and particularly relates to Ti 2 C 3 A para-aramid nano-fiber electromagnetic shielding composite material and a preparation method thereof.
Background
Along with the rapid development of the electronic information industry, various electrical equipment such as computers, televisions, microwave ovens, mobile phone signal towers and the like are integrated in the aspects and moments of life of people, and the equipment provides convenient and efficient life for people and brings new and serious electromagnetic pollution problems. Relevant researches show that electromagnetic waves generated by electronic equipment such as mobile phones and computers in life not only endanger the health of people constantly and increase the probability of the people suffering from diseases such as leukemia, but also interfere the normal work of precision equipment to cause accidents, thereby causing irreparable economic loss. Therefore, in order to reduce and avoid the adverse effects of electromagnetic pollution and electromagnetic interference on our lives, a material capable of effectively shielding the electromagnetic pollution is developed, and the material has important economic benefits and social significance.
At present, most of electromagnetic shielding materials are made of metal and metal composite materials, and the electromagnetic shielding materials have good electromagnetic shielding efficiency, but have the problems of high density, corrosion resistance, heavy use, difficulty in adjusting the efficiency and low electromagnetic wave absorption efficiency in a broadband range of 8-18 GHz, so that the development and further application of the electromagnetic shielding materials are limited. Two-dimensional transition metal carbide Ti 2 C 3 Is a novel ceramic-like nanomaterial with a graphene-like structure, which was discovered in 2011 in cooperation with professor Gogotsi and professor barsum of the university of Drexel, usa. Due to the characteristics of self-lubrication, high toughness, conductivity and the like, Ti 2 C 3 The method is widely used for research in the fields of energy storage, catalysis, adsorption, sensors, electromagnetic shielding, novel polymer reinforced matrix composite materials and the like. And Ti 3 AlC 2 Ti prepared by etching with hydrofluoric acid or by etching with a mixed system of hydrochloric acid and lithium fluoride 2 C 3 Has hydrophilicity, metal conductivity and excellent electrochemical performance, and is one excellent nanometer electromagnetic shielding material. The para-aramid fiber is chemically poly-p-phenylene terephthalamide (PPTA), is a network-like cross-linked high polymer, has excellent properties of high strength, high modulus, high temperature resistance, corrosion resistance and the like, and is widely applied to the fields of aerospace, electric traffic, national defense and military and the like. The para-Aramid fiber is specially treated to obtain para-Aramid Nanofiber, the English name of the para-Aramid Nanofiber, namely ANF, is used for short, and the ANF is subjected to vacuum-assisted filtration to obtain a film material with high strength and high toughness, so that the film material is a base material and a reinforcing phase nano polymer material with excellent performances.
In order to overcome the disadvantages of the existing electromagnetic shielding material, the performance of the electromagnetic shielding composite material needs to be further optimized, however, Ti is added 2 C 3 And para-aramid nanofibers have not been reported.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides Ti 2 C 3 The product is light in weight, high in conductivity, high in shielding efficiency, simple and convenient to operate, and capable of being produced in large scale, and provides reference for electromagnetic shielding research of electronic products.
The invention is realized by the following technical scheme:
ti 2 C 3 The preparation method of the electromagnetic shielding composite material of the para-aramid nano-fiber comprises the following steps,
step 1, adding Ti 2 C 3 Mixing the dispersion liquid and the para-aramid nano-fiber dispersion liquid and then carrying out ultrasonic treatment to obtain a mixed system A, wherein the mass of the para-aramid nano-fiber is Ti 2 C 3 And 3% -9% of the total mass of the para-aramid nano-fiber;
step 2, sequentially carrying out vacuum-assisted filtration and hot-pressing drying on the mixed system A to obtain Ti 2 C 3 The electromagnetic shielding composite material of/para-aramid nano-fiber.
Preferably, the pressure of the vacuum-assisted filtration in step 2 is 0.6 to 0.8 MPa.
Preferably, the hot-pressing drying in the step 2 is carried out at 100-200 ℃ for 20-30 min.
Preferably, the ultrasonic time in the step 1 is 30min to 60 min.
Preferably, the para-aramid nanofiber dispersion liquid in the step 1 is obtained by the following steps,
step 1, adding potassium hydroxide and para-aramid fiber in a mass ratio of 0.75-1.5 into a dimethyl sulfoxide solution to obtain a mixed system B;
and 2, stirring the mixed system B until the color of the mixed system B is dark red.
Further, the mixing system B in the step 2 is stirred at the stirring speed of 300 r/min-400 r/min at the temperature of 20-30 ℃.
Preferably, Ti as described in step 1 2 C 3 The dispersion is purified before being mixed with the para-aramid nanofiber dispersion until the dispersion is dark green.
Further, said Ti 2 C 3 The dispersion liquid is purified by centrifuging for 10min to 60min at the rotating speed of 4000r/min to 9000 r/min.
Still further, said Ti 2 C 3 The dispersion is obtained in the following manner,
ti of 200 meshes to 400 meshes 3 AlC 2 Adding the mixture into a mixed system consisting of lithium fluoride and hydrochloric acid, and magnetically stirring the mixture for 24 to 48 hours at the temperature of between 35 and 40 ℃.
Ti prepared by any one of the above methods 2 C 3 A para-aramid nano-fiber composite material.
Compared with the prior art, the invention has the following beneficial technical effects:
ti of the invention 2 C 3 The preparation method of the electromagnetic shielding composite material of the/para-aramid nano-fiber selects Ti 2 C 3 And para-aramid nanofibers as raw materials, wherein Ti 2 C 3 Is a main material of electromagnetic shielding, and utilizes the advantages of easy dispersion, easy film formation and reinforced performance of the para-aramid nano-fiber when the mass of the para-aramid nano-fiber is less than that of Ti 2 C 3 And when the mass of the para-aramid nano-fiber is more than 3 percent of the total mass of the Ti, the synthesized composite material has small mechanical strength and is difficult to form a film 2 C 3 And 9 percent of the total mass of the para-aramid nano-fiber, the synthesized composite material has conductivityPoor energy and can not achieve the effect of realizing high-efficiency electromagnetic shielding, so that the para-aramid nano-fiber has the mass of Ti 2 C 3 And the total mass of the para-aramid nano-fiber is 3-9%, vacuum-assisted filtration can ensure that the electromagnetic shielding composite material forms a microscopic layered structure, so that the electromagnetic shielding performance is improved through multiple reflection and absorption, hot-press drying can ensure that the mechanical strength of the composite material is improved under the condition of not changing the physical properties of the material, so that two raw materials are well subjected to interface combination, certain electrical conductivity is ensured, the strength of the material is improved, the electromagnetic shielding performance is regulated and controlled, and reference is provided for electromagnetic shielding research of electronic products.
Further, potassium hydroxide and para-aramid fibers are added into the dimethyl sulfoxide solution and stirred until the color of the mixed system B is dark red, and the para-aramid nanofiber dispersion liquid obtained by adopting a chemical splitting method has the characteristics of nano-scale dimension, uniform dispersion of a water phase and high chemical reactivity.
Further, Ti 3 AlC 2 Adding the mixture into a mixed system consisting of lithium fluoride and hydrochloric acid, magnetically stirring the mixture for 24 to 48 hours to obtain Ti by adopting a chemical etching method 2 C 3 The dispersion liquid has the characteristics of two-dimensional layered nano structure, water phase dispersion and long-time stability of the dispersion liquid.
Drawings
FIG. 1 shows Ti prepared in example 1 of the present invention 2 C 3 The dispersion and tyndall effect are shown.
FIG. 2 shows Ti prepared in example 1 of the present invention 2 C 3 Material and raw material Ti 3 AlC 2 Comparative XRD patterns.
FIG. 3 shows Ti prepared by the present invention 2 C 3 a/ANF-3 electromagnetic shielding composite material object graph.
FIG. 4 shows Ti prepared by the present invention 2 C 3 SEM image of/ANF-3 electromagnetic shielding composite material section.
FIG. 5 shows Ti prepared by the present invention 2 C 3 And (3) an electromagnetic shielding performance graph of the/ANF composite material.
Detailed Description
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
The invention combines nano ceramic material Ti 2 C 3 And ANF, respectively, from Ti 2 C 3 The composite material is compounded with ANF, and the electromagnetic shielding composite material with light weight, high strength, high shielding effectiveness and flexibility is prepared by a vacuum auxiliary filtering method, so that a new idea is provided for solving the problem of electromagnetic compatibility of high-end instruments and equipment, and a reference is provided for the electromagnetic shielding research of electronic products.
The invention relates to a Ti 2 C 3 The preparation method of the/ANF electromagnetic shielding composite material comprises the following steps,
step 1, according to 1 g: 1 g: 20ml of Ti with 200 meshes to 400 meshes 3 AlC 2 Adding lithium fluoride into hydrochloric acid solution with the mass fraction of 37%, magnetically stirring and reacting for 24-48 h at the temperature of 35-40 ℃, and preparing unpurified Ti by chemical etching 2 C 3 A dispersion liquid;
step 2, the unpurified Ti obtained in the step 1 is processed 2 C 3 Putting the dispersion into a centrifugal tube, centrifuging the dispersion for 10-60 min in a centrifuge at the rotating speed of 4000-9000 r/min by using deionized water or distilled water, separating and removing chemical reaction byproducts until the dispersion is dark green, and obtaining cleaned and purified Ti 2 C 3 Adding Ti to the mixture with deionized water 2 C 3 5mg/ml to 10mg/ml of dispersion is prepared, the dispersion is stable in state and does not settle or delaminate within 10 days;
step 3, adding potassium hydroxide and para-aramid fibers into a dimethyl sulfoxide solution according to the mass ratio of 0.75-1.5, stirring at the stirring speed of 300-400 r/min at the temperature of 20-30 ℃ for 7-9 days, wherein the solution is dark red, and diluting 50mL of ANF dispersion liquid to 400mL with deionized water for later use to obtain 0.25mg/mL of ANF dispersion liquid;
step 4, mixing the ANF dispersion liquid prepared in the step 3 and the Ti prepared in the step 2 2 C 3 Mixing the dispersion liquid, and mixingSound dispersion is carried out for 30 min-60 min to obtain evenly dispersed Ti 2 C 3 Mixed solution of ANF, wherein the ANF is ANF and Ti 2 C 3 3-9% of the total mass;
step 5, Ti prepared in the step 4 is added 2 C 3 The mixed solution of/ANF is firstly filtered under vacuum assistance under 0.6MPa to 0.8MPa, and then is dried under hot pressing at 100 ℃ to 200 ℃ for 20min to 30min to obtain Ti 2 C 3 the/ANF electromagnetic shielding composite material.
Example 1
Ti 2 C 3 The preparation method of the/ANF electromagnetic shielding composite material comprises the following steps,
step 1, 1g of 400 mesh Ti 3 AlC 2 1g of lithium fluoride is added into hydrochloric acid solution with the volume of 20ml and the mass fraction of 37 percent, the mixture is magnetically stirred and reacted for 24 hours at the temperature of 35 ℃ and the speed of 400r/min, and unpurified Ti is obtained by chemical etching 2 C 3 A dispersion liquid;
step 2, obtaining unrefined Ti in the step 1 2 C 3 Putting the dispersion liquid into a centrifugal tube, centrifuging for 20min at the rotating speed of 4000r/min, separating and removing by-products of chemical etching reaction until the dispersion liquid is dark green, and obtaining purified Ti after cleaning 2 C 3 ，Ti 2 C 3 And raw material Ti 3 AlC 2 The comparative XRD pattern is shown in FIG. 2, from which FIG. 2 Ti can be seen 2 C 3 To obtain higher purity, the Ti is treated with deionized water 2 C 3 The resulting dispersion was prepared into a stable dispersion of 5mg/ml, the Tyndall effect of red light is shown in FIG. 1, and Ti produced can be seen from FIG. 1 2 C 3 The size is in the nanometer level and the water phase is dispersed uniformly;
step 3, adding potassium hydroxide and para-aramid fibers into a dimethyl sulfoxide solution according to the mass ratio of 3:2, stirring for a week at 25 ℃ and at a stirring speed of 400r/min, taking 50mL of ANF dispersion liquid, diluting the ANF dispersion liquid to 400mL with deionized water for later use, and obtaining 0.25mg/mL of ANF dispersion liquid;
step 4, mixing the ANF dispersion liquid prepared in the step 3 with the ANF dispersion liquid prepared in the step 2Prepared Ti 2 C 3 Mixing the dispersion liquid, and performing ultrasonic dispersion for 30min to obtain uniformly dispersed Ti 2 C 3 Mixed solution of ANF, wherein the ANF is ANF and Ti 2 C 3 3% of the total mass;
step 5, Ti prepared in the step 4 2 C 3 The mixed solution of/ANF is filtered under vacuum assistance under 0.8MPa, and then is dried under hot pressing at 105 ℃ for 30min, thus obtaining Ti with 3 percent of ANF mass fraction 2 C 3 The composite material of this example is Ti 2 C 3 ANF-3, as shown in FIG. 3, from FIG. 3 it can be seen that Ti 2 C 3 ANF-3 is in the form of black flakes, and Ti 2 C 3 SEM image of/ANF-3 cross section is shown in FIG. 4, the filamentous substance is ANF, and ANF is uniformly bonded to Ti 2 C 3 The layered structure can reflect and absorb for multiple times, and Ti is improved 2 C 3 Electromagnetic shielding performance of/ANF.
Example 2
Ti 2 C 3 The preparation method of the/ANF electromagnetic shielding composite material comprises the following steps,
step 1, mixing 1g of 400 mesh Ti 3 AlC 2 1g of lithium fluoride is added into hydrochloric acid solution with the volume of 20ml and the mass fraction of 37 percent, the mixture is magnetically stirred and reacted for 24 hours at the temperature of 35 ℃ and the speed of 400r/min, and unpurified Ti is obtained by chemical etching 2 C 3 A dispersion liquid;
step 2, unpurified Ti obtained in the step 1 2 C 3 Loading the dispersion into a centrifuge tube, centrifuging at 4000r/min for 20min, separating to remove by-product of chemical etching reaction until the dispersion is dark green, and collecting cleaned and purified Ti 2 C 3 Adding Ti to the mixture with deionized water 2 C 3 Preparing a stable dispersion of 7.5 mg/ml;
step 3, adding potassium hydroxide and para-aramid fibers into a dimethyl sulfoxide solution according to the mass ratio of 3:2, stirring for a week at 25 ℃ and at a stirring speed of 400r/min, taking 50mL of ANF dispersion liquid, diluting the ANF dispersion liquid to 400mL with deionized water for later use, and obtaining 0.25mg/mL of ANF dispersion liquid;
step 4, mixing the ANF dispersion liquid prepared in the step 3 and the Ti prepared in the step 2 2 C 3 Mixing the dispersion liquid, and performing ultrasonic dispersion for 30min to obtain uniformly dispersed Ti 2 C 3 Mixed solution of ANF, wherein the ANF is ANF and Ti 2 C 3 6% of the total mass;
step 5, Ti prepared in the step 4 is added 2 C 3 The mixed solution of/ANF is filtered under vacuum assistance under 0.8MPa, and then is dried under hot pressing at 105 ℃ for 30min, thus obtaining Ti with the mass fraction of 6 percent of ANF 2 C 3 The composite material of this example is Ti 2 C 3 /ANF-6。
Example 3
Ti 2 C 3 The preparation method of the ANF electromagnetic shielding composite material comprises the following steps,
step 1, mixing 1g of 400 mesh Ti 3 AlC 2 1g of lithium fluoride is added into hydrochloric acid solution with the volume of 20ml and the mass fraction of 37 percent, the mixture is magnetically stirred and reacted for 24 hours under the conditions of 35 ℃ and 400r/min, and unpurified Ti is obtained by chemical etching 2 C 3 A dispersion liquid;
step 2, unpurified Ti obtained in the step 1 2 C 3 Loading the dispersion into a centrifuge tube, centrifuging at 4000r/min for 20min, separating to remove by-product of chemical etching reaction until the dispersion is dark green, and cleaning to obtain purified Ti 2 C 3 Adding Ti to the mixture with deionized water 2 C 3 Preparing a stable dispersion of 10 mg/ml;
step 3, adding potassium hydroxide and para-aramid fiber into a dimethyl sulfoxide solution according to the mass ratio of 3:2, stirring for a week at 25 ℃ and at a stirring speed of 400r/min, wherein the solution is dark red, and diluting 50mL of ANF dispersion liquid to 400mL of deionized water for later use to obtain 0.25mg/mL of ANF dispersion liquid;
step 4, mixing the ANF dispersion liquid prepared in the step 3 and the Ti prepared in the step 2 2 C 3 Mixing the dispersion liquid, and ultrasonically dispersing 3Uniformly dispersed Ti is obtained in 0min 2 C 3 Mixed solution of ANF, wherein the ANF is ANF and Ti 2 C 3 9% of the total mass;
step 5, Ti prepared in the step 4 2 C 3 The mixed solution of/ANF is filtered under vacuum pressure of 0.8MPa, and then hot-pressed and dried for 30min at 105 ℃, so that Ti with the mass fraction of 9 percent of ANF can be obtained 2 C 3 The composite material of this example is Ti 2 C 3 /ANF-9。
Example 4
Ti 2 C 3 The preparation method of the/ANF electromagnetic shielding composite material comprises the following steps,
step 1, adding 1g of 200-mesh Ti 3 AlC 2 Adding into a mixed system of 1g of lithium fluoride and 20ml of hydrochloric acid solution with the mass fraction of 37%, magnetically stirring and reacting for 48h at 40 ℃ and 400r/min, and obtaining unrefined Ti by chemical etching 2 C 3 A dispersion liquid;
step 2, obtaining unrefined Ti in the step 1 2 C 3 Loading the dispersion into a centrifugal tube, centrifuging at 4000r/min for 60min, separating to remove by-products of chemical etching reaction until the dispersion is dark green, and cleaning to obtain purified Ti 2 C 3 Adding Ti to the mixture with deionized water 2 C 3 Preparing a stable dispersion of 5 mg/ml;
step 3, adding potassium hydroxide and para-aramid fiber into a dimethyl sulfoxide solution according to the mass ratio of 3:4, stirring at the stirring speed of 400r/min at 30 ℃ for 9 days, wherein the solution is dark red, and diluting 50mL of ANF dispersion liquid to 400mL of deionized water for later use to obtain 0.25mg/mL of ANF dispersion liquid;
step 4, mixing the ANF dispersion liquid prepared in the step 3 and the Ti prepared in the step 2 2 C 3 Mixing the dispersion liquid, and performing ultrasonic dispersion for 60min to obtain uniformly dispersed Ti 2 C 3 /ANF mixture, wherein the mass of ANF is ANF and Ti 2 C 3 4% of the total mass;
step 5, the step4 prepared Ti 2 C 3 The mixed solution of/ANF is filtered under vacuum pressure of 0.8MPa, and then hot-pressed and dried for 30min at 200 ℃ to obtain Ti with ANF mass fraction of 4% 2 C 3 The ANF electromagnetic shielding composite material is Ti 2 C 3 /ANF-4。
Example 5
Ti 2 C 3 The preparation method of the/ANF electromagnetic shielding composite material comprises the following steps,
step 1, 1g of 300 mesh Ti 3 AlC 2 Adding into a mixed system of 1g of lithium fluoride and 20ml of hydrochloric acid solution with the mass fraction of 37%, magnetically stirring and reacting for 36h at 37 ℃ and 400r/min, and obtaining unrefined Ti by chemical etching 2 C 3 A dispersion liquid;
step 2, unpurified Ti obtained in the step 1 2 C 3 Putting the dispersion into a centrifugal tube, centrifuging for 30min at the rotating speed of 6500r/min, separating and removing by-products of the chemical etching reaction until the dispersion is dark green, and obtaining purified Ti after cleaning 2 C 3 Adding Ti to the mixture with deionized water 2 C 3 Preparing a stable dispersion of 7.5 mg/ml;
step 3, adding potassium hydroxide and para-aramid fiber into a dimethyl sulfoxide solution according to the mass ratio of 1:1, stirring for 8 days at the temperature of 25 ℃ and at the stirring speed of 350r/min, wherein the solution is dark red, and diluting 50mL of ANF dispersion liquid to 400mL of deionized water for later use to obtain 0.25mg/mL of ANF dispersion liquid;
step 4, the ANF dispersion liquid prepared in the step 3 and the Ti prepared in the step 2 are mixed 2 C 3 Mixing the dispersion liquid, and performing ultrasonic dispersion for 45min to obtain uniformly dispersed Ti 2 C 3 Mixed solution of ANF, wherein the ANF is ANF and Ti 2 C 3 7% of the total mass;
step 5, Ti prepared in the step 4 is added 2 C 3 The mixed solution of/ANF is filtered under vacuum pressure of 0.7MPa, and then hot-pressed and dried for 25min at 150 ℃, so that Ti with 7 percent of ANF mass fraction is obtained 2 C 3 The composite material of this example is Ti 2 C 3 /ANF-7。
Example 6
Ti 2 C 3 The preparation method of the ANF electromagnetic shielding composite material comprises the following steps,
step 1, mixing 1g of 400 mesh Ti 3 AlC 2 Adding into a mixed system of 1g of lithium fluoride and 20ml of hydrochloric acid solution with the mass fraction of 37%, magnetically stirring and reacting for 24h at the temperature of 35 ℃ and the speed of 400r/min, and obtaining unrefined Ti by chemical etching 2 C 3 A dispersion liquid;
step 2, obtaining unrefined Ti in the step 1 2 C 3 The dispersion liquid is put into a centrifuge tube and centrifuged for 10min at the rotating speed of 9000r/min, by-products of chemical etching reaction are separated and removed until the dispersion liquid presents dark green, and purified Ti after cleaning is obtained 2 C 3 Adding Ti to the mixture with deionized water 2 C 3 Preparing a stable dispersion of 10 mg/ml;
step 3, adding potassium hydroxide and para-aramid fiber into a dimethyl sulfoxide solution according to the mass ratio of 3:2, stirring for a week at the temperature of 20 ℃ and the stirring speed of 300r/min, wherein the solution is dark red, and diluting 50mL of ANF dispersion liquid to 400mL of deionized water for later use to obtain 0.25mg/mL of ANF dispersion liquid;
step 4, the ANF dispersion liquid prepared in the step 3 and the Ti prepared in the step 2 are mixed 2 C 3 Mixing the dispersion liquid, and performing ultrasonic dispersion for 30min to obtain uniformly dispersed Ti 2 C 3 /ANF mixture, wherein the mass of ANF is ANF and Ti 2 C 3 8% of the total mass;
step 5, Ti prepared in the step 4 is added 2 C 3 The mixed solution of/ANF is filtered under vacuum pressure of 0.6MPa, and then hot-pressed and dried at 100 ℃ for 20min to obtain Ti with ANF mass fraction of 8% 2 C 3 The composite material of this example is Ti 2 C 3 /ANF-8。
Next, the electromagnetic shielding composite materials prepared in examples 1 to 3 of the present invention were examined,
first, the electrical properties,
adopts a multifunctional digital four-probe tester with the model number of ST-2258C to test the electromagnetic shielding composite material Ti 2 C 3 /ANF-3、Ti 2 C 3 ANF-6 and Ti 2 C 3 the/ANF-9 was tested for electrical properties, 3 times per sample and the results averaged. As shown in Table 1, it can be seen that the electrical conductivity of the composite material reached 2226.96S/cm when the weight percentage of ANF was 3%, 1976.90S/cm when the weight percentage of ANF was 6%, and 1006.19S/cm when the weight percentage of ANF was 9%, and these data indicate that ANF was uniformly dispersed in Ti 2 C 3 Compared with other electromagnetic shielding composite materials, the composite material has high conductivity.
Secondly, the electromagnetic shielding performance is improved,
according to the national standard GJB 6190-2008, adopting a vector network analyzer which is produced by Agilent and has the model number of PNA-N5244A, and adopting a waveguide method to measure the electromagnetic shielding composite material Ti 2 C 3 /ANF-3、Ti 2 C 3 ANF-6 and Ti 2 C 3 The electromagnetic shielding performance of/ANF-9, the size of the sample prepared before measurement is 22.9mm x 10.2mm, the test frequency is 8.2 GHz-12.4 GHz, and the electromagnetic shielding performance data obtained finally are shown in the electromagnetic shielding performance column in Table 1 and FIG. 2, wherein the electromagnetic shielding performance in Table 1 is characterized by SE (12.4GHz, dB).
TABLE 1Ti 2 C 3 Parameter related to/ANF electromagnetic shielding composite material
Figure BDA0002033828500000111
As can be seen from the data of conductivity, electromagnetic shielding performance and electromagnetic shielding performance of the composite material of FIG. 5 in Table 1, Ti in the present invention 2 C 3 the/ANF electromagnetic shielding composite material has good conductive performance, outstanding and adjustable shielding performance, and is an excellent electromagnetic shielding composite material.
The invention relates to a Ti 2 C 3 The electromagnetic shielding composite material of/para-aramid nano fiber is prepared by selecting Ti of ternary lamellar carbide MAX phase 3 AlC 2 And para-aramid fiber as raw material, and chemically etching Ti by using a mixed system consisting of hydrochloric acid solution and lithium fluoride 3 AlC 2 To obtain Ti 2 C 3 Dispersing, treating para-aramid fiber with mixed system of dimethyl sulfoxide and potassium hydroxide to obtain para-aramid nanofiber dispersion, and adding Ti 2 C 3 Carrying out ultrasonic dispersion on the dispersion liquid and the ANF dispersion liquid, and then carrying out vacuum-assisted filtration and hot-pressing drying to obtain Ti 2 C 3 The ANF electromagnetic shielding composite material has the characteristics of simple preparation process, easiness in mass production, low density, excellent conductivity and electromagnetic shielding performance.

Claims (4)

1. Ti 2 C 3 The preparation method of the electromagnetic shielding composite material of the para-aramid nano-fiber is characterized by comprising the following steps of,
step 1, adding Ti 2 C 3 Mixing the dispersion liquid and the para-aramid nano-fiber dispersion liquid, and performing ultrasonic treatment to obtain a mixed system A, wherein the mass of the para-aramid nano-fiber is Ti 2 C 3 And 3% -9% of the total mass of the para-aramid nano-fiber;
the para-aramid nano-fiber dispersion liquid is obtained by the following steps,
step 1a, adding potassium hydroxide and para-aramid fiber in a mass ratio of 0.75-1.5 into a dimethyl sulfoxide solution to obtain a mixed system B;
step 1B, stirring the mixed system B until the color of the mixed system B is dark red;
the Ti 2 C 3 Centrifuging the dispersion liquid for 10-60 min at the rotating speed of 4000-9000 r/min until the dispersion liquid is dark green before mixing the dispersion liquid with the para-aramid nano-fiber dispersion liquid, and then using deionized water to remove Ti 2 C 3 The concentration of the dispersion is adjusted to 5mg/ml to 10mg/ml, Ti 2 C 3 Dispersing liquid is according toIs obtained in the following manner by the use of,
ti of 200 meshes to 400 meshes 3 AlC 2 Adding the mixture into a mixed system consisting of lithium fluoride and hydrochloric acid, and magnetically stirring the mixture for 24 to 48 hours at the temperature of between 35 and 40 ℃;
step 2, carrying out vacuum auxiliary filtration on the mixed system A at 0.6-0.8 MPa, and carrying out hot-pressing drying at 100-200 ℃ for 20-30 min to obtain Ti 2 C 3 The electromagnetic shielding composite material of/para-aramid nano-fiber.
2. A Ti according to claim 1 2 C 3 The preparation method of the para-aramid nanofiber electromagnetic shielding composite material is characterized in that the ultrasonic time in the step 1 is 30-60 min.
3. A Ti according to claim 1 2 C 3 The preparation method of the/para-aramid nano-fiber electromagnetic shielding composite material is characterized in that the mixed system B in the step 1B is stirred at the stirring speed of 300 r/min-400 r/min at the temperature of 20-30 ℃.
4. Ti prepared by the method of any one of claims 1 to 3 2 C 3 A/para-aramid nano-fiber composite material.
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